The pomegranate (Punica granatum), especially its fruit, possesses a vast ethnomedical history and represents a phytochemical reservoir of heuristic medical value. The tree and fruit can be divided into several anatomical compartments, and the fruit juice, peel and oil are known to be weakly estrogenic and heuristically of interest for treatment of menopausal symptoms and sequellae. In this study, analysis of estrogen in pomegranate extract was carried out with LC/MS/MS. Three batches of pomegranate extract samples were used to analysis the target compounds (estrogen). The contents of estrogen derivatives in the samples were 38.6 ppb of estriol, 83.5 ppb of estrone,and 10.9 ppb of estradiol. This result suggests that the pomegranate extract can used for treatment of menopause symptoms in the woman.

As the human mixed saliva plays important roles for the protection, regeneration, immunity, and molecular transfer/ signaling in the oral and gastro-intestinal mucosa, the salivary contents have great implications for the general health of human body. Nevertheless, the analysis method of human saliva has not been well developed up to date, because the proteins of mixed saliva are rapidly interacted with each other and easily degraded by proteolytic enzymes and microorganisms. This study aims to develop an immunoprecipitation-based high performance liquid chromatography (IP-HPLC) for the analysis of human mixed saliva. The representative IP-HPLC analyses were performed to compare among different subjects in variable general conditions. Compared to the normal control the subjects suffered from bacterial infections of gastro-intestinal enteritis, chronic periodontitis, and acute necrotizing gingivo-stomatitis showed dramatic increase of LL-37 level depending on the severity of diseases, while the subject suffered from Herpes stomatitis, a viral infection showed great increase of β-defensin 2. These data indicate that LL-37 in human mixed saliva is more responsible to the bacterial infections of gastro-intestinal enteritis, chronic periodontitis, and acute necrotizing gingivo-stomatitis, while β-defensin 2 is more responsible to the viral infection of Herpes stomatitis. This study also suggeststhat the IP-HPLC be easily applicable to the wide range of biological samples for the quantitative analysis of an objective protein.

본 논문에서는 식품 중 퀴놀론계(QNs) 합성항균제(marbofloxacin, norfloxacin, danofloxacin, ciprofloxacin, enrofloxacin, difloxacin, sarafloxacin, oxolinic acid 그리고 flumequine) 9종을 분석하기 위하여, 액-액 추출 과정을 거쳐서 형광검출기가 장착된 액체크로마토그래피를 이용하여 QNs를 효율적으로 동시분석하는 방법을 확립하였다. 컬럼은 Zorbax Eclipse XDB-C8(150 mm×4.6 mm, 5 μm), 이동상 용매는 200 mM ammonium acetate buffer (pH 4.5)와 ACN로 기울기 용리를 사용하였으며, 유속은 1.5 ml/min, 그리고, 주입량은 10 μl로 설정하여 분석하였다. 확립 된 분석조건으로, 표준검정 곡선은 10-500 μg/kg의 농도범위에서 상관계수가 0.9989 이상의 양호한 직선성을 나타내었으며, 회수율은 50, 100 그리고 500 μg/kg의 농도에서 89.6-106.5 %로, 향상된 추출효율을 나타내었다. 검출한계는 1-16 μg/kg이었고, 정량한계는 3-47 μg/kg이었으며, 일내(intra-day)와 일간(inter-day) 정밀도(CV%)는 0.2-15.0 %, 0.5-11.7 %이었다. 따라서, 확립된 분석방법은 광어 및 계란 중의 QNs을 효과적으로 분석하는데 이용될 수 있을 것으로 사료된다.

HPLC에 의한 주요 aflatoxins(afatoxin B₁, B₂, G₁ 및 G₂)의 동시 분석에서 postcolumn 유도체화법을 시도하였다. Electrochemical cell(Kobra-cell)을 사용한 postcolumn 유도체화법은 기존의 precolumn 유도체화법보다 분석시간을 단축하였으며(약 1/2 단축), 더 안전하고, 향상된 분석능을 보였다. Aflatoxin B₁과 G₁의 경우 10~100 ppb에서, 그리고 B₂와 G₂의 경우 3~30 ppb에서 직선성을 나타내었다. Aflatoxin B₁과 G₁은 각각 88.9% 및 100.5%로 양호환 회수육을 보였다. Aflatoxin B₂와 G₂의 경우 분리도는 우수하였으나 회수율에 있어서 변이가 크게 나타났다.

Triacylglycerols of the seeds of Ginkgo biloba have been resolved by high-performace liquid chromatography(HPLC in the silver-ion and reverse-phase modes. The fatty acids were identified by a combination of capillary gas chromatography and gas-chromatography /mass spectrometry as the methyl and /or picolinyl ester. The main components are C18:2Ω6(39.0mol%), C18:1Ω7(asclepic acid 21.5mol%), and C18:1Ω9(oleic acid, 13.8mol%). Considerable amounts of unusual acid such as C20:3δ5,11,14 (5.7mol%), C18:2δ5,9(2.8mol%), and C18:3δ5,9,12(1.6mol%), were checked. In addition, an anteiso-branched fatty acid, 14-methylhexadecanoic acid, was also present as a minor component(0.9 mol%). The triacylglycerols were separated into 17 fractions by reverse-phase HPLC, and the fractionation was achieved according to the partition numnber(PN) in which a δ5-non methylene interrupted double bond(5-NMDB) showed different behaviour from a methylene interrupted double bond in a molecule with a given cahinlength. Silver-ion HPLC exhibited excellent resolution in which fractions(23 fractions) were resolved on the basis of the number and configuration of double bonds. In this instance, the strength of interaction of a δ5-NMDB system with silver ions seemed to be weaker than a methylene interrupted double bond system. The principal triacylglycerol species are as follows ; (C18:2Ω6)2/C18:1Ω7, C18:1Ω9/C18:1Ω7/C18:2Ω6, (C18:1Ω7)2/C18:2Ω6, C16:1Ω7/C18:1Ω9/C20:3δ5,11,14, C16:1Ω7/C18:1Ω7/C20:3δ5,11,14, C18:1Ω9/C18:1Ω7/C18:2Ω6, C18:1Ω9/C18:2δ5,5/C20:3δ5,11,14, (C18:1Ω7)2/C18:2Ω6 and (C18:1Ω9)2/C18:2Ω6, while simple triacylglycerols without C18:2Ω6)3 were not present. Stereospecific analysis showed that fatty acids with δ5-NMDB system and saturated chains were predominantly located at the site of sn-3 carbon of glycerol backbones. It is evident that there is asymmetry in the distribution of fatty acids in the TG molecules of Ginkgo nut oils.

Sulfonamides, a therapeutically important group of antimicrobial drugs, are widely used to treat and prevent the acute systemic and skin infections in dairy cattle. They also pose an economic hazard through inhibition of growth of dairy starter cultures. This study was carried out to compare four screening methods for detection of sulfamethazine in milk and determine the positive milk sample by HPLC method. Sulfamethazine was used to spike at five levels of sulfamethazine. The Lac-Tek test and CharmII test were also consistent better than TTCII test and Delvo SP test in sulfamethazine detection. Analysis probabilities of obtaining a positive response with TTCII test and Delvo SP test assay at 50 ppb sulfamethazine level in milk samples were only 14%, 42% each. Whereas using the Lac-Tek test and CharmII test would have resulted in 100% identification of the five levels. Determination of sufamethazine using the HPLC method in the spiked milk were 10.64, 19.30, 30.76, 38.83 and 50.23 ppb, respectively.

The possibilities for HPLC analysis of lipids have been revolutionised by the availability of evaporative light-scattering detectors, with which the response is independent of the nature of the mobile phase and does not depend On the presence of specific chromophores in the lipids. It was thus possible to develop an HPLC procedure, involving ternary gradient elution, for separating all the lipid classes in animal tissues in a single step. Although reversed-phase HPLC has been widely used for the analysis of molecular species of lipids, sliver ion chromatography can be a valuable alternative. For example, a stable silver ion column for HPLC was developed which permitted resolution of molecular species of triacylglycerols, even from such complex samples as fish oils, again With light-scattering detection and gradient elution. The capacity for HPLC resolution of diastereomeric diacyl-sn-glycerol derivatives, prepared from triacylglycerols. has lead to a new simple method for stereospecific analysis of the latter.

The fast separation and determination of cefatrizine·propylene glycol and inmpurities - TACA: 7-amino-3-(1,2,3-triazol-4-yl)thiomethyl-3-cephem-4-carboxylic acid and 7-ACA; 7-amino cephalosporanic acid - was performed by the high poerformance liquid chromatography using octadecyl siland (ODS) column. Methanol and ammonium phosphate buffer [0.03M(NH4)2 HPO4, (pH 7.5)] was used analyze, as eluent. The experimental value of the contents of cefatrizine·propylene glycol and impurities agree with the theoretical value of those.

The analytical method for 16 organophosphorus pesticides was developed in this study. The 16 organophosphorus pesticides were analyzed by liquid chromatography-tandem mass spectrometry (LC/MS/MS) using on-line solid phase extraction (on-line SPE) with PLRP- S cartridge. Analysis of all analytes in the MS/MS was processed in the electrospray ioni-zation (ESI) positive mode. They are Azinphos ethyl, Chlorfenvinphos, Ethion, Famphur, Phosmet, Phosphamidon, Terbufos, Aspon, Chlorpyrifos-methyl, Crotoxyphos, Dichlofenthi-on, Dicrotophos, Fonofos, Thionazin, Dimethoate and Iprobenfos. Limits of detection (LODs) and Limits of quantification(LOQs) were obtained as 0.8~2.0 ng/L and 2.6~6.4 ng/L, respectively. All compounds were not detected at the 8 sampling points of the raw water and clean water.

본 연구에서는 합성보존제로 흔히 쓰이는 메칠파라벤과 방부효능을 가지는 천연추출성분인 p-아니식애씨드를 HPLC를 통해 분리분석 하는 방법을 개발하였다. 메칠파라벤과 p-아니식애씨드는 같은 분자량(152.15 g/mol)과 비슷한 구조, 같은 최대흡수파장(250 nm)을 보이기 때문에 HPLC로 분석 시 동일한 RT값(13.3 min)을 갖는다. 본 연구 저자들은 아세틸화 반응을 통해 메칠파라벤을 선택적으로 유도체화 한 후 C18 컬럼을 통해 분석했을 때 두 물질이 분리됨을 확인하였다. 아세틸화반응을 거치면서 메칠파라벤의 피크유지시간이 13.3 min에서 23.9 min으로 이동하였으며, 평균값은 23.9±0.1min, 피크면적 값은 5042882±4778로 일정하게 나타났다. 또한 직선성의 평가에서 결정계수값은 0.9999658로 1에 가까운 값을 보였다. 시료의 검출한계는 1.47μg/mL이었고 정량한계는 4.44μg/mL이었다. 결론적으로 본 연구를 통해 개발된 분석법은 화장품 분야에서 유사한 구조를 가진 보존제 분석에 유용하게 사용될 수 있을 것으로 기대된다.